The Effect of Fly Ash Composition and Reaction Conditions on Hydrothermal Synthesis of Zeolitic Materials

Fly ash 조성(組成)과 반응조건(反應條件)이 zeolite성(性) 물질(物質)의 열수합성(熱水合成)에 미치는 영향(影響)

  • Choi, Choong-Lyeal (Department of Agricultural Chemistry, Kyungpook National University) ;
  • Lee, Dong-Hoon (Department of Agricultural Chemistry, Kyungpook National University) ;
  • Park, Man (Department of Industrial Chemistry, Kyungpook National University) ;
  • Choi, Jyung (Department of Agricultural Chemistry, Kyungpook National University)
  • 최충렬 (경북대학교 농화학과) ;
  • 이동훈 (경북대학교 농화학과) ;
  • 박만 (경북대학교 공업화학과) ;
  • 최정 (경북대학교 농화학과)
  • Published : 1999.03.30

Abstract

This study was performed to examine the effect of initial composition ratio and various reaction conditions on CEC and crystallinity of the product in hydrothermal synthesis of zeolitic materials from fly ash. Na-P1 zeolite was formed from the mixture with $SiO_2/Al_2O_3$ ratio above 2.55, however from the mixture with $SiO_2/Al_2O_3$ ratio below 2.25 hydroxy sodalite was formed. The CEC of reaction product(Na-P1 zeolite) treated with 3N-NaOH, $Na_2O/Al_2O_3$ ratio 2.55 and $SiO_2/Al_2O_3$ ratio 2.0 for 12 hours at $103^{\circ}C$ was about $285cmol^+kg^{-1}$, which was higher than those of the products of other reaction condition. The crystallinity of Na-P1 zeolite as high as 45.1% was attained at the optimum reaction condition of 2N-NaOH, $SiO_2/Al_2O_3$ ratio 2.55, $Na_2O/Al_2O_3$ ratio 1.5 for 12 hours at $103^{\circ}C$. The XRD peak of the reaction product could be measured at 7.16, 5.04, 4.12, 3.18, $2.69{\AA}$ and tetragonal pillar shape observed by SEM image be characteristic for Na-P1 zeolite. Judging from the result, it should be considered the optimum synthesis condition for Na-P1 zeolite from fly ash was 2~3N NaOH, $SiO_2/Al_2O_3$ ratio 2.55 and $Na_2O/Al_2O_3$ ratio 1.5~2.0 for 12 hours at $80{\sim}103^{\circ}C$.

Fly ash를 이용(利用)한 zeolite성(性) 물질(物質)의 열수합성(熱水合成)에 있어서 반응재료(反應材料)의 초기구성성분(初期構成成分) 비율(比率)과 여러가지 반응조건(反應條件)이 반응생성물(反應生成物)의 CEC및 결정화도(結晶化度)에 미치는 영향(影響)과 최적반응조건(最適反應條件)을 조사(調査)하였다. $SiO_2/Al_2O_3$ 비율(比率)이 2.55이상(以上)에서는 Na-P1 zeolite가 생성(生成)되었으나, 2.25이하(以下)에서는 hydroxy sodalite가 생성(生成)되었다. 3N-NaOH, $SiO_2/Al_2O_3$ 비율(比率) 2.55, $Na_2O/Al_2O_3$ 비율(比率) 2.0, $103^{\circ}C$에서 12시간(時間) 처리(處理)한 반응생성물(反應生成物)의 CEC 가 $285cmol^+kg^{-1}$으로 다른 반응조건(反應條件)의 생성물(生成物)보다 높았으며, 결정화도(結晶化度)는 2N-NaOH, $SiO_2/Al_2O_3$ 비율(比率) 2.55 $Na_2O/Al_2O_3$ 비율(比率) 2.0, $103^{\circ}C$에서 12시간(時間) 처리(處理)한 반응생성물(反應生成物)이 45.1%로서 가장 높게 나타났다. 반응생성물(反應生成物)의 $SiO_2/Al_2O_3$ 비율(比率)은 fly ash 보다 낮았으며, ignition loss는 결품격자(結品格子) 내(內)의 흡착수(吸着水)에 의해 4.0%로 증가(增加)하였다. 반응생성물(反應生成物)의 XRD peak와 전자현미경사진(電子顯微鏡寫眞)으로 관찰(觀察)한 결과(結果) Na-P1 zeolite의 특징(特徵)을 나타내었다. Fly ash를 이용(利用)한 Na-P1 zeolite의 최적(最適) 열수합성조건(熱水合成條件)은 NaOH 농도(濃度) 2~3N, $SiO_2/Al_2O_3$, 2.55, $Na_2O/Al_2O_3$ 비율(比率) 1.5~2.0, 반응온도(反應溫度) $80{\sim}103^{\circ}C$, 반응시간(反應時間)은 12시간(時間) 이상(以上)으로 판단(判斷)된다.

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